CN115074172B - Lubricating grease and preparation method thereof - Google Patents

Lubricating grease and preparation method thereof Download PDF

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Publication number
CN115074172B
CN115074172B CN202110261751.9A CN202110261751A CN115074172B CN 115074172 B CN115074172 B CN 115074172B CN 202110261751 A CN202110261751 A CN 202110261751A CN 115074172 B CN115074172 B CN 115074172B
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grease
base oil
formula
silole
thickener
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CN115074172A (en
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刘欣阳
庄敏阳
郑会
刘中其
姜靓
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/04—Mixtures of base-materials and additives
    • C10M169/048—Mixtures of base-materials and additives the additives being a mixture of compounds of unknown or incompletely defined constitution, non-macromolecular and macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/065—Sulfides; Selenides; Tellurides
    • C10M2201/066—Molybdenum sulfide
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/02—Hydroxy compounds
    • C10M2207/023—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
    • C10M2207/026—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings with tertiary alkyl groups
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28—Esters
    • C10M2207/283—Esters of polyhydroxy compounds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
    • C10M2215/064—Di- and triaryl amines
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
    • C10M2215/064—Di- and triaryl amines
    • C10M2215/065—Phenyl-Naphthyl amines
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/08—Amides
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/22—Heterocyclic nitrogen compounds
    • C10M2215/223—Five-membered rings containing nitrogen and carbon only
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2217/04—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2217/045—Polyureas; Polyurethanes
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/046—Overbasedsulfonic acid salts
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/06—Thio-acids; Thiocyanates; Derivatives thereof
    • C10M2219/062—Thio-acids; Thiocyanates; Derivatives thereof having carbon-to-sulfur double bonds
    • C10M2219/066—Thiocarbamic type compounds
    • C10M2219/068—Thiocarbamate metal salts
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/04—Phosphate esters
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/04—Phosphate esters
    • C10M2223/045—Metal containing thio derivatives
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
    • C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
    • C10M2223/04—Phosphate esters
    • C10M2223/047—Thioderivatives not containing metallic elements
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2227/00—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
    • C10M2227/08—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions having metal-to-carbon bonds
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)

Abstract

The invention provides lubricating grease and a preparation method thereof. The lubricating grease comprises, by mass, 0.01% -10% of silole derivatives, 50% -95% of base oil, 3% -40% of thickening agents, 0.01% -3% of rust inhibitors, 0-2% of antioxidants and 0-3% of extreme pressure agents; the structure of the silole derivative is shown as a formula (I):

Description

Lubricating grease and preparation method thereof
Technical Field
The invention relates to lubricating grease, in particular to servo system lubricating grease with good antioxidant performance and extreme pressure antiwear performance.
Background
The grease is a solid-to-semi-fluid product prepared by dispersing a thickening agent in a liquid lubricant, has lubricating, protecting and sealing functions, and is widely applied to industrial machinery, agricultural machinery, transportation industry, aerospace industry, electronic information industry and various military equipment.
Grease is critical for long-term reliable operation of mechanical components in harsh environments. Some equipped servo systems have higher requirements on high and low temperature, rotating speed and load, and lubricating grease is required to have excellent extreme pressure wear resistance. Therefore, development of grease with excellent extreme pressure antiwear performance is still a development direction for those skilled in the art.
Disclosure of Invention
The invention provides lubricating grease and a preparation method thereof.
The lubricating grease comprises, by mass, 0.01% -10% of silole derivatives, 50% -95% of base oil, 3% -40% of thickening agents, 0.01% -3% of rust inhibitors, 0-2% of antioxidants and 0-3% of extreme pressure agents; the structure of the silole derivative is shown as a formula (I):
Figure BDA0002970325280000011
wherein each R 0 Are identical or different from each other and are each independently selected from hydrogen, C 1-6 Straight or branched hydrocarbon radicals (preferably hydrogen, C 1-4 Linear or branched alkyl), each x is independently selected from integers between 0 and 5 (preferably 0, 1,2, 3); the L' group is selected from
Figure BDA0002970325280000012
C 1-6 Straight-chain or branched hydrocarbon radicals (preferably->
Figure BDA0002970325280000013
C 1-4 Linear or branched alkyl), wherein R 0 Selected from hydrogen, C 1-6 Straight or branched hydrocarbon radicals (preferably hydrogen, C 1-4 Linear or branched alkyl), x is selected fromAn integer between 0 and 5 (preferably 0, 1,2, 3);
n is an integer between 1 and 10 (preferably an integer between 1 and 5); n a groups, equal to or different from each other, are each independently selected from the group consisting of a residue of a terpene or a residue of a sulphurised terpene (preferably a residue of a sulphurised terpene);
the radical L being a single bond or a (n+1) -valent C 1-30 Hydrocarbyl radicals (preferably single bond or (n+1) valent C 1-6 Linear or branched alkyl).
According to the present invention, examples of the terpene residue or the terpene sulfide residue include a residue obtained by removing one hydrogen atom from a terpene or a terpene sulfide. The terpenes include monoterpenes, sesquiterpenes, diterpenes, triterpenes, tetraterpenes, and polyterpenes, such as myrcene, p-menthane, biotan, farnesol, farnesyl ester, menthol, camphor, vitamin A, carotene, squalene, nerol, citral, camphene, pinane, pinene, borneol, mountain years, abietic acid, lutein, and lycopene. The vulcanized terpene is a sulfide of the terpene, and can be, for example, laurene sulfide, menthane sulfide, biotan sulfide, farnesol sulfide, farnesyl sulfide, menthol sulfide, camphor sulfide, vitamin A sulfide, carotene sulfide, squalene sulfide, nerol sulfide, citral sulfide, camphene sulfide, pinane sulfide, pinene sulfide, borneol sulfide, mountain year sulfide, abietic acid sulfide, lutein sulfide, lycopene sulfide.
According to the invention, the silole derivative may be one or more of the following compounds:
Figure BDA0002970325280000021
according to the present invention, the method for producing a silole derivative comprises a step of reacting a silole compound represented by the formula (II) with a compound represented by the formula (III),
Figure BDA0002970325280000022
in formula (II), each R 0 Are identical or different from each other and are each independently selected from hydrogen, C 1-6 Straight or branched hydrocarbon radicals (preferably hydrogen, C 1-4 Linear or branched alkyl), each x is independently selected from integers between 0 and 5 (preferably 0, 1,2, 3); the L' group is selected from
Figure BDA0002970325280000031
C 1-6 Straight-chain or branched hydrocarbon radicals (preferably->
Figure BDA0002970325280000032
C 1-4 Linear or branched alkyl), wherein R 0 Selected from hydrogen, C 1-6 Straight or branched hydrocarbon radicals (preferably hydrogen, C 1-4 Linear or branched alkyl) x is selected from integers between 0 and 5 (preferably 0, 1,2, 3);
in formula (III), the X group is F, cl, br, I or OH (preferably Cl, br); n is an integer between 1 and 10 (preferably an integer between 1 and 5); n a groups, equal to or different from each other, are each independently selected from the group consisting of a residue of a terpene or a residue of a sulphurised terpene (preferably a residue of a sulphurised terpene); the radical L being a single bond or a (n+1) -valent C 1-30 Hydrocarbyl radicals (preferably single bond or (n+1) valent C 1-6 Linear or branched alkyl).
According to the method for producing a silole derivative of the present invention, as the residue of terpene or the residue of vulcanized terpene, for example, a group obtained by removing one hydrogen atom from terpene or vulcanized terpene can be mentioned. The terpenes include monoterpenes, sesquiterpenes, diterpenes, triterpenes, tetraterpenes, and polyterpenes, such as myrcene, p-menthane, biotan, farnesol, farnesyl ester, menthol, camphor, vitamin A, carotene, squalene, nerol, citral, camphene, pinane, pinene, borneol, mountain years, abietic acid, lutein, and lycopene. The vulcanized terpene is a sulfide of the terpene, and can be, for example, laurene sulfide, menthane sulfide, biotan sulfide, farnesol sulfide, farnesyl sulfide, menthol sulfide, camphor sulfide, vitamin A sulfide, carotene sulfide, squalene sulfide, nerol sulfide, citral sulfide, camphene sulfide, pinane sulfide, pinene sulfide, borneol sulfide, mountain year sulfide, abietic acid sulfide, lutein sulfide, lycopene sulfide.
According to the preparation method of the silole derivative, the silole compound shown in the formula (II) can be selected from one or more of the following compounds:
Figure BDA0002970325280000033
according to the preparation method of the silole derivative, the compound shown in the formula (III) can be selected from one or more of the following compounds:
Figure BDA0002970325280000034
according to the method for producing a silole derivative of the present invention, in the reaction, the molar ratio between the silole compound represented by formula (II) and the compound represented by formula (III) is preferably 1:0.5 to 5, most preferably 1:0.8 to 1.2.
According to the process for the preparation of a silole derivative according to the invention, the reaction temperature is preferably between 0 and 50 ℃, preferably between 15 and 35 ℃.
According to the preparation method of the silole derivative, the reaction time is preferably 6-96 hours, preferably 12-72 hours.
According to the process for the preparation of a silole derivative according to the invention, a catalyst is preferably added to the reaction. The catalyst is preferably one or more of a metal phosphine complex, a metal halide and a hydrocarbyl phosphine compound, more preferably a mixture of a metal phosphine complex, a metal halide and a hydrocarbyl phosphine compound, and the molar ratio of the three is preferably 1:0.1 to 10:0.1 to 10, more preferably 1:0.2 to 5:0.2 to 5.
According to the preparation method of the silole derivative, preferably, the structure of the metal phosphine complex is
Figure BDA0002970325280000041
Wherein M is Pd, ru or Rh, L is selected from PPh 3 Ph, F, cl, br, I. The metal phosphine complex may be selected from one or more of tetrakis (triphenylphosphine) palladium, tris (triphenylphosphine) palladium chloride, bis (triphenylphosphine) palladium dichloride, tris (triphenylphosphine) palladium trichloride, tetrakis (triphenylphosphine) ruthenium, tris (triphenylphosphine) ruthenium chloride, bis (triphenylphosphine) ruthenium dichloride, tris (triphenylphosphine) ruthenium trichloride, tetrakis (triphenylphosphine) rhodium, tris (triphenylphosphine) rhodium chloride, bis (triphenylphosphine) rhodium dichloride and (triphenylphosphine) rhodium trichloride, preferably one or more of tetrakis (triphenylphosphine) palladium, tris (triphenylphosphine) palladium chloride, bis (triphenylphosphine) palladium dichloride and (triphenylphosphine) palladium trichloride.
According to the method for producing a silole derivative of the present invention, preferably, the metal halide may be one or more of copper halide, iron halide and zinc halide, for example, one or more of copper chloride, cuprous chloride, cupric bromide, cuprous bromide, cupric iodide, cuprous iodide, ferric chloride, ferrous chloride, ferric bromide, ferrous bromide, ferric iodide, ferrous iodide, zinc chloride, zinc bromide, zinc iodide and zinc iodide, more preferably, one or more of copper chloride, cuprous chloride, cupric bromide, cuprous bromide, cupric iodide and cuprous iodide.
According to the method for producing a silole derivative of the present invention, preferably, the hydrocarbyl phosphine compound has the structure of
Figure BDA0002970325280000042
Wherein each R is independently selected from C 6 ～C 10 Aryl and C of (2) 1 ～C 6 Wherein at least one R is C 6 ～C 10 Aryl groups of (a). The C is 6 ～C 10 The aryl group of (a) may be selected from phenyl, naphthyl; the C is 1 ～C 6 The linear or branched alkyl group of (a) may be selected from methyl, ethyl, propyl, isopropyl, butyl, isobutyl, pentyl, isopentyl, hexyl or isohexyl. The hydrocarbyl phosphine compound may be selected fromTriphenylphosphine, diphenylbutylphosphine are used.
According to the preparation method of the silole derivative, the addition amount of the catalyst is preferably 1-20% of the mass of the silole compound shown in the formula (II).
According to the method for producing a silole derivative of the present invention, preferably, a solvent is added to the reaction. The solvent is preferably C 1 ～C 10 For example, methylamine, dimethylamine, trimethylamine, ethylamine, diethylamine, triethylamine, propylamine, dipropylamine, tripropylamine, tetrahydrofuran, most preferably C 1 ～C 10 The volume ratio of the organic amine to the furan is preferably 1:0.1 to 10. The solvent may be removed after the completion of the reaction by a method known in the art, and is not particularly limited, and the removal method includes a method of distillation, evaporation, column chromatography.
According to the preparation method of the silole derivative, preferably, the silole derivative is separated and purified by a column chromatography method, a mixed solvent of dichloromethane/petroleum ether can be used as an eluent, and the volume ratio of the dichloromethane to the petroleum ether is preferably 1:0.5 to 5.
The silole derivative has excellent photoluminescence performance and oxidation resistance, can emit yellow-green fluorescence under ultraviolet irradiation, and can be applied to luminous components and devices, fluorescent probes, biological imaging, lubricating oil and lubricating grease.
According to the present invention, the base oil may be one or more of mineral oil, vegetable oil and synthetic oil, preferably synthetic oil. The synthetic oil may be one or more selected from poly alpha-olefin, alkyl naphthalene and ester oil, and the examples may include one or more selected from PAO4, PAO6, PAO8, PAO10, alkyl naphthalene, diisooctyl sebacate and trimethylolpropane ester.
According to the invention, the thickener comprises one or more of a polyurea thickener, a lithium-based thickener, a composite lithium-based thickener, a sodium amide soap thickener, a calcium-based thickener and a composite aluminum-based thickener, preferably one or more of a polyurea thickener, a lithium-based thickener, a composite lithium-based thickener, a sodium amide soap thickener and a composite aluminum-based thickener, and most preferably a composite lithium-based thickener and/or a sodium amide soap thickener.
According to the invention, the rust inhibitor can be benzooxazoles and/or sulfonate rust inhibitors. Examples of the rust inhibitor include one or more of benzotriazole, barium petroleum sulfonate, sodium petroleum sulfonate and barium basic dinonylnaphthalene sulfonate.
According to the present invention, the extreme pressure agent may be selected from one or more of organo molybdenum, dialkyl dithiocarbamate and amino-thio ester, and examples may include one or more of molybdenum oxy sulfide di (2-ethylhexyl) dithiophosphate, molybdenum disulfide, tricresyl phosphate, phenyl thiophosphate and dibutyl dithiocarbamic acid.
According to the present invention, the antioxidant may be an amine antioxidant and/or a phenolic antioxidant, and examples include one or more of diphenylamine, alkylated diphenylamine, N-phenyl-alpha naphthylamine, 2, 6-di-t-butyl-p-cresol and 2, 6-di-t-butyl-4-hydroxyphenyl acrylate.
According to the invention, optionally, the lubricating grease comprises, by mass, 0.1% -5% of a silole derivative, 75% -90% of base oil, 8% -20% of a thickening agent, 0.1% -2.5% of an anti-rust agent, 0.01% -1% of an antioxidant and 0.01% -2% of an extreme pressure agent.
The preparation method of the lubricating grease comprises the following steps: mixing and refining base oil, a thickening agent and the silole derivative, then mixing with the antirust agent, the antioxidant and the extreme pressure agent, and grinding into grease. The temperature of the refining operation is 160-240 ℃, preferably 180-220 ℃; the refining operation takes 10 to 240min, preferably 20 to 60min. The whole base oil, the silole derivative and the thickening agent can be mixed and refined together, or after part of the base oil, the silole derivative and the thickening agent are mixed and refined, the mixture is mixed with the rest of the base oil, the rust inhibitor, the antioxidant and the extreme pressure agent.
According to the preparation method of the lubricating grease, the composite lithium-based lubricating grease can be prepared by selecting the composite lithium-based thickening agent.
According to the preparation method of the lubricating grease, the preparation method of the composite lithium-based lubricating grease comprises the following steps: mixing and heating part of base oil, fatty acid and small molecular acid in a reaction kettle, heating to 40-100 ℃, adding the water solution of the silole derivative and lithium hydroxide, heating to remove water, continuously heating to 190-220 ℃ for high-temperature refining, adding the rest of base oil, cooling to 60-120 ℃, adding the antirust agent, the antioxidant and the extreme pressure agent, and grinding into grease. The fatty acid is C 12 ～C 20 Fatty acids and/or C 12 ～C 20 Hydroxy fatty acid, which can be one or more of lauric acid, palmitic acid, stearic acid and 12-hydroxy stearic acid; the small molecule acid is C 2 ～C 11 The organic acid of (2) can be one or more of acetic acid, propionic acid, oxalic acid, adipic acid, azelaic acid, sebacic acid and terephthalic acid. The equivalent ratio between the fatty acid and the small molecule acid may be 1:1 to 4:1, preferably 1.5:1 to 3:1. The ratio between the sum of the equivalents of fatty acid and small molecule acid and the equivalent of lithium hydroxide may be from the prior art, for example, 1:1 to 1:2.
According to the preparation method of the lubricating grease, the amide sodium soap thickener is selected to prepare the amide sodium soap-based lubricating grease.
According to the preparation method of the lubricating grease, the preparation method of the sodium amide soap-based lubricating grease comprises the following steps: mixing and refining base oil, an amide sodium soap thickener and the silole derivative, mixing with the antirust agent, the antioxidant and the extreme pressure agent, and grinding into grease. The temperature of the refining operation is 160-240 ℃, preferably 180-220 ℃; the refining operation takes 10 to 240min, preferably 20 to 60min. All the base oil, the silole derivative and the amide sodium soap thickener can be mixed and refined together, or part of the base oil, the silole derivative and the amide sodium soap thickener can be mixed and refined and then mixed with the rest of the base oil, the rust inhibitor, the antioxidant and the extreme pressure agent.
According to the grease preparation method of the present invention, preferably, the silole derivative is dissolved in a solvent in advance. The solvent is preferably aromatic hydrocarbon solvent, for example, benzene, toluene and xylene, and the weight of the solvent is 0.5-100 times (preferably 1-20 times) of that of the silole derivative.
The lubricating grease provided by the invention has excellent photoluminescence performance, rust resistance, oxidation resistance and extreme pressure wear resistance, and is suitable for servo systems of equipment.
Detailed Description
In the context of the present specification, the term "single bond" is sometimes used in the definition of a group. By "single bond" is meant that the group is absent. For example, assume the structural formula-CH 2 -A-CH 3 Wherein the group A is defined as selected from single bonds and methyl groups. In view of this, if A is a single bond, this means that the group A is absent, in which case the formula is correspondingly reduced to-CH 2 -CH 3 。
In the context of the present specification, the expression "number +valence +group" or the like means a group obtained by removing the number of hydrogen atoms represented by the number from a basic structure (such as a chain, a ring, or a combination thereof, etc.) to which the group corresponds, preferably a group obtained by removing the number of hydrogen atoms represented by the number from carbon atoms (preferably saturated carbon atoms and/or non-identical carbon atoms) contained in the structure. For example, "3-valent linear or branched alkyl group" refers to a group obtained by removing 3 hydrogen atoms from a linear or branched alkane (i.e., the basic chain to which the linear or branched alkyl group corresponds), while "2-valent linear or branched heteroalkyl group" refers to a group obtained by removing 2 hydrogen atoms from a linear or branched heteroalkane (preferably from a carbon atom contained in the heteroalkane, or further from a non-identical carbon atom). For example, the 2-valent propyl group may be-CH 2 -CH 2 -CH 2 -*、
Figure BDA0002970325280000071
The 3-valent propyl group can be
Figure BDA0002970325280000072
The 4-valent propyl group can be +.>
Figure BDA0002970325280000073
Wherein represents the binding end in the group that can be bonded to other groups.
The main raw materials used are as follows:
chemical reagents such as 1-alkynyl-1, 2,3,4, 5-pentathizole, bromosulfurated terpene, cuprous iodide, triphenylphosphine, tetraphenylphosphine palladium, octadecylamine, MDI, 12-hydroxystearic acid, stearic acid, benzoic acid, lithium hydroxide monohydrate, aluminum isopropoxide trimer, tetrahydrofuran, triethylamine, dichloromethane, petroleum ether and the like are obtained from carbofuran reagent company, inokai reagent company or sigma reagent company; the PAO10 base oil is from the Ekkimex company; additives such as diphenylamine, 2, 6-di-tert-butyl-p-cresol, benzotriazole, molybdenum di (2-ethylhexyl) dithiophosphate and the like are from Van der Waals trade Limited or New Country Ruifeng New Material Co., ltd.
Preparation of sodium amide soap thickener
Refluxing 1mol of dimethyl terephthalate and 1mol of octadecylamine in dimethylformamide for 8 hours at 150 ℃, adding 1mol of sodium hydroxide for saponification for 4 hours, evaporating to remove the solvent, and then washing and drying the solvent to obtain the sodium amide soap thickener.
Example 1
1mmol of 1-alkynyl-1, 2,3,4, 5-penta-phenylsilole, 1.2mmol of bromosulfurated terpene, 0.1mmol of cuprous iodide and 0.1mmol of triphenylphosphine were placed in a 100mL Schlenk reaction flask, 0.02mmol of tetraphenylphosphine palladium, 30mL of tetrahydrofuran/triethylamine (2/1, v/v) were added under nitrogen protection, and the mixture was reacted at room temperature for 48 hours. After the reaction, filtering and spin-drying the filtrate, and separating and purifying the product by column chromatography with a mixed solvent of dichloromethane/petroleum ether (1/2, v/v) as an eluent to obtain a yellow solid product with the yield of 65%. The mass spectrum results of the product were: MS (MALDI-TOF): m/z calcd:698.2[ M ]] + ,found:698.2。
The reaction scheme for example 1 is shown below:
Figure BDA0002970325280000081
example 2
1mmol of 1-methyl-1-alkynyl-2, 3,4, 5-tetraphenylsilole, 1.2mmol of bromosulfurated terpene, 0.1mmol of cuprous iodide and 0.1mmol of triphenylphosphine were placed in a 100mL Schlenk reaction flask, and 0.02mmol of triphenylphosphine palladium, 30mL of tetrahydrofuran/triethylamine (2/1, v/v) were added under nitrogen protection, and the mixture was reacted at room temperature for 48 hours. After the reaction, the mixture was filtered and the filtrate was dried by spin-drying, and the product was purified by column chromatography using a mixed solvent of dichloromethane/petroleum ether (1/2, v/v) as an eluent to give a yellow solid product in 69% yield. The mass spectrum results of the product were: MS (MALDI-TOF): m/z calcd:636.2[ M ]] + ,found:636.2。
The reaction scheme of example 2 is shown below:
Figure BDA0002970325280000091
example 3
300 g of PAO10 base oil, 43.59 g of 12-hydroxystearic acid and 14.61g of sebacic acid are mixed and heated to 85 ℃ in a reaction kettle, 5 g of the product of the example 1 is dissolved in 10 g of toluene and then added into the reaction kettle, 13.37 g of lithium hydroxide monohydrate is mixed with 60 g of distilled water and heated to 95 ℃, after all lithium hydroxide is dissolved, the mixture is added into the reaction kettle, heating and dewatering are continued, heating to 210 ℃, 140 g of PAO10 base oil is added, cooling to 120 ℃,5 g of benzotriazole is added, and grinding is carried out after cooling to room temperature to obtain grease.
Example 4
300 g of PAO10 base oil, 43.59 g of 12-hydroxystearic acid and 14.61g of sebacic acid are mixed and heated to 85 ℃ in a reaction kettle, 15 g of the product of the example 1 is dissolved in 30 g of toluene and then added into the reaction kettle, 13.37 g of lithium hydroxide monohydrate is mixed with 60 g of distilled water and heated to 95 ℃, after all lithium hydroxide is dissolved, the mixture is added into the reaction kettle, heating and dewatering are continued, heating to 210 ℃, 140 g of PAO10 base oil is added, cooling to 120 ℃,5 g of benzotriazole is added, and grinding is carried out after cooling to room temperature to obtain grease.
Example 5
300 g of PAO10 base oil, 43.59 g of 12-hydroxystearic acid and 14.61g of sebacic acid are mixed and heated to 85 ℃ in a reaction kettle, 25 g of the product of the example 1 is dissolved in 50 g of toluene and then added into the reaction kettle, 13.37 g of lithium hydroxide monohydrate is mixed with 60 g of distilled water and heated to 95 ℃, after all lithium hydroxide is dissolved, the mixture is added into the reaction kettle, heating and dewatering are continued, heating to 210 ℃, 140 g of PAO10 base oil is added, cooling to 120 ℃,5 g of benzotriazole is added, and grinding is carried out after cooling to room temperature to obtain grease.
Example 6
300 g of PAO10 base oil, 43.59 g of 12-hydroxystearic acid and 14.61g of sebacic acid are mixed and heated to 85 ℃ in a reaction kettle, 15 g of the product of the example 2 is dissolved in 30 g of toluene and then added into the reaction kettle, 13.37 g of lithium hydroxide monohydrate is mixed with 60 g of distilled water and heated to 95 ℃, after all lithium hydroxide is dissolved, the mixture is added into the reaction kettle, heating and dewatering are continued, heating to 210 ℃, 140 g of PAO10 base oil is added, cooling to 120 ℃, 2.5 g of diphenylamine and 5 g of benzotriazole are added, and grinding is carried out after cooling to room temperature to obtain grease.
Example 7
300 g of PAO10 base oil, 43.59 g of 12-hydroxystearic acid and 14.61g of sebacic acid are mixed and heated to 85 ℃ in a reaction kettle, 15 g of the product of the example 2 is dissolved in 30 g of toluene and then added into the reaction kettle, 13.37 g of lithium hydroxide monohydrate is mixed with 60 g of distilled water and heated to 95 ℃, after all lithium hydroxide is dissolved, the mixture is added into the reaction kettle, heating and dewatering are continued, heating to 210 ℃, 140 g of PAO10 base oil is added, cooling to 120 ℃, 10 g of molybdenum oxide dithiophosphate and 5 g of benzotriazole are added, and grinding is carried out after cooling to room temperature to obtain grease.
Example 8
300 g of PAO10 base oil, 43.59 g of 12-hydroxystearic acid and 14.61g of sebacic acid are mixed and heated to 85 ℃ in a reaction kettle, 15 g of the product of the example 2 is dissolved in 30 g of toluene and then added into the reaction kettle, 13.37 g of lithium hydroxide monohydrate is mixed with 60 g of distilled water and heated to 95 ℃, after all lithium hydroxide is dissolved, the mixture is added into the reaction kettle, heating and dewatering are continued, heating to 210 ℃, 140 g of PAO10 base oil is added, cooling to 120 ℃, 2.5 g of diphenylamine, 10 g of molybdenum oxide di (2-ethylhexyl) dithiophosphate and 5 g of benzotriazole are added, and the mixture is ground into grease after cooling to room temperature.
Comparative example 1
300 g of PAO10 base oil, 43.59 g of 12-hydroxystearic acid and 14.61g of sebacic acid are mixed and heated to 85 ℃ in a reaction kettle, 13.37 g of lithium hydroxide monohydrate and 60 g of distilled water are mixed and heated to 95 ℃, the mixture is added into the reaction kettle after the lithium hydroxide is completely dissolved, the mixture is heated and dehydrated and then is continuously heated to 210 ℃, 140 g of PAO10 base oil is added, the mixture is cooled to 120 ℃,5 g of benzotriazole is added, and the mixture is ground into grease after the mixture is cooled to room temperature.
Comparative example 2
300 g of PAO10 base oil, 43.59 g of 12-hydroxystearic acid and 14.61g of sebacic acid are mixed and heated to 85 ℃ in a reaction kettle, 13.37 g of lithium hydroxide monohydrate and 60 g of distilled water are mixed and heated to 95 ℃, the mixture is added into the reaction kettle after the lithium hydroxide is completely dissolved, the mixture is heated and dehydrated and then is continuously heated to 210 ℃, 140 g of PAO10 base oil is added, the mixture is cooled to 120 ℃,5 g of diphenylamine and 5 g of benzotriazole are added, and the mixture is ground into grease after the mixture is cooled to room temperature.
Comparative example 3
300 g of PAO10 base oil, 43.59 g of 12-hydroxystearic acid and 14.61g of sebacic acid are mixed and heated to 85 ℃ in a reaction kettle, 13.37 g of lithium hydroxide monohydrate and 60 g of distilled water are mixed and heated to 95 ℃, the mixture is added into the reaction kettle after the lithium hydroxide is completely dissolved, the mixture is heated and dehydrated and then is continuously heated to 210 ℃, 140 g of PAO10 base oil is added, the mixture is cooled to 120 ℃, 10 g of molybdenum oxide dithiophosphate and 5 g of benzotriazole are added, and the mixture is ground into grease after the mixture is cooled to room temperature.
Performance of the greases of examples 3,4,5, 6, 7, 8, 1,2,3 was evaluated by GB/T3498, GB/T269, SH/T0719, SH/T0325, SH/T0324, SH/T0202, SH/T0204, and the evaluation results are shown in Table 1.
Table 1 evaluation results
Figure BDA0002970325280000111
Example 9
300 g of PAO10 base oil and 75 g of amide sodium soap thickener are mixed in a reaction kettle and heated to 90 ℃,5 g of the product of the example 1 is dissolved in 10 g of toluene and then added into the reaction kettle, after 30 minutes, the mixture is heated to remove water and is continuously heated to 210 ℃ for 20 minutes, 125 g of PAO10 base oil is added and cooled to 120 ℃,5 g of benzotriazole is added, and after the mixture is cooled to room temperature, the mixture is ground into grease.
Example 10
300 g of PAO10 base oil and 75 g of amide sodium soap thickener are mixed in a reaction kettle and heated to 90 ℃, 15 g of the product of the example 1 is dissolved in 30 g of toluene and then added into the reaction kettle, after 30 minutes, the mixture is heated to remove water and is continuously heated to 210 ℃ for 20 minutes, 125 g of PAO10 base oil is added and cooled to 120 ℃,5 g of benzotriazole is added, and after the mixture is cooled to room temperature, the mixture is ground into grease.
Example 11
300 g of PAO10 base oil and 75 g of amide sodium soap thickener are mixed in a reaction kettle and heated to 90 ℃, 25 g of the product of the example 1 is dissolved in 50 g of toluene and then added into the reaction kettle, after 30 minutes, the mixture is heated to remove water and is continuously heated to 210 ℃ for 20 minutes, 125 g of PAO10 base oil is added and cooled to 120 ℃,5 g of benzotriazole is added, and after the mixture is cooled to room temperature, the mixture is ground into grease.
Example 12
300 g of PAO10 base oil and 75 g of amide sodium soap thickener are mixed and heated to 90 ℃ in a reaction kettle, 15 g of the product of the example 1 is dissolved in 30 g of toluene and then added into the reaction kettle, water is removed by heating after 30 minutes, the temperature is kept constant at 210 ℃ for 20 minutes, 125 g of PAO10 base oil is added and cooled to 120 ℃,5 g of 2, 6-di-tert-butyl-p-cresol, 10 g of molybdenum oxide dithiophosphate and 5 g of benzotriazole are added, and the mixture is ground into grease after cooling to room temperature.
Example 13
300 g of PAO10 base oil and 75 g of amide sodium soap thickener are mixed and heated to 90 ℃ in a reaction kettle, 5 g of the product of the example 2 is dissolved in 30 g of toluene and then added into the reaction kettle, water is removed by heating after 30 minutes, the temperature is kept constant at 210 ℃ for 20 minutes, 125 g of PAO10 base oil is added and cooled to 120 ℃,5 g of 2, 6-di-tert-butyl-p-cresol and 5 g of benzotriazole are added, and the mixture is ground into grease after being cooled to room temperature.
Example 14
300 g of PAO10 base oil and 75 g of amide sodium soap thickener are mixed and heated to 90 ℃ in a reaction kettle, 15 g of the product of the example 2 is dissolved in 30 g of toluene and then added into the reaction kettle, water is removed by heating after 30 minutes, the temperature is kept constant at 210 ℃ for 20 minutes, 125 g of PAO10 base oil is added and cooled to 120 ℃, 10 g of molybdenum oxide di (2-ethylhexyl) dithiophosphate and 5 g of benzotriazole are added, and the mixture is ground into grease after being cooled to room temperature.
Comparative example 4
300 g of PAO10 base oil and 75 g of amide sodium soap thickener are mixed and heated to 90 ℃ in a reaction kettle, water is removed by heating after 30 minutes, the temperature is kept constant for 20 minutes after the temperature is continuously raised to 210 ℃, 125 g of PAO10 base oil is added and cooled to 120 ℃,5 g of benzotriazole is added, and the mixture is ground into grease after the mixture is cooled to room temperature.
Comparative example 5
300 g of PAO10 base oil and 75 g of amide sodium soap thickener are mixed and heated to 90 ℃ in a reaction kettle, water is removed by heating after 30 minutes, the temperature is kept constant at 210 ℃ for 20 minutes, 125 g of PAO10 base oil is added and cooled to 120 ℃,5 g of 2, 6-di-tert-butyl-p-cresol and 5 g of benzotriazole are added, and the mixture is ground into grease after cooling to room temperature.
Comparative example 6
300 g of PAO10 base oil and 75 g of amide sodium soap thickener are mixed and heated to 90 ℃ in a reaction kettle, water is removed by heating after 30 minutes, the temperature is kept constant for 20 minutes after the temperature is continuously raised to 210 ℃, 125 g of PAO10 base oil is added and cooled to 120 ℃, 10 g of molybdenum oxide dithiophosphate and 5 g of benzotriazole are added, and the mixture is ground into grease after the mixture is cooled to room temperature.
Performance of the greases of examples 9, 10, 11, 12, 13, 14, 4,5 and 6 were evaluated according to GB/T3498, GB/T269, SH/T0719, SH/T0325, SH/T0324, SH/T0202 and SH/T0204, and the evaluation results are shown in Table 2.
Table 2 evaluation results
Figure BDA0002970325280000131

Claims (16)

1. The lubricating grease comprises, by mass, 0.01% -10% of a silole derivative, 50% -95% of base oil, 3% -40% of a thickening agent, 0.01% -3% of an antirust agent, 0-2% of an antioxidant and 0-3% of an extreme pressure agent; wherein the structure of the silole derivative is shown as a formula (I):
Figure FDA0004140482570000011
wherein each R 0 Are identical or different from each other and are each independently selected from hydrogen, C 1-4 A linear or branched alkyl group, each x is independently selected from 0, 1,2, 3; the L' group is selected from phenyl and methyl;
n is 1; the A group is selected from the residues of sulphurised terpenes; the residue of the sulfurated terpene is a group obtained by removing one hydrogen atom from the sulfurated terpene; the radical L being C of (n+1) valence 1-6 A linear alkyl group.
2. Grease according to claim 1, wherein the structure of the silole derivative is:
Figure FDA0004140482570000012
3. the grease of claim 1, wherein the method for producing a silole derivative comprises a step of reacting a silole compound represented by the formula (II) with a compound represented by the formula (III),
Figure FDA0004140482570000013
in formula (II), each R 0 Are identical or different from each other and are each independently selected from hydrogen, C 1-4 A linear or branched alkyl group, each x is independently selected from 0, 1,2, 3; the L' group is selected from phenyl and methyl; in the formula (III), X groups are Cl and Br; n is 1; the A group is selected from the residues of sulphurised terpenes; the radical L being C of (n+1) valence 1-6 A linear alkyl group.
4. A grease according to claim 3, wherein the residue of the sulphurised terpene is a group obtained by removing a hydrogen atom from a sulphurised terpene.
5. A grease according to claim 3, wherein the silole compound of formula (II) is selected from one or more of the following:
Figure FDA0004140482570000021
or the compound shown in the formula (III) is selected from one or more of the following compounds:
Figure FDA0004140482570000022
6. a grease according to claim 3, wherein in the reaction the molar ratio between the silole compound of formula (II) and the compound of formula (III) is 1:0.5 to 5; the temperature of the reaction is 0-50 ℃.
7. A grease according to claim 3, wherein in the reaction the molar ratio between the silole compound of formula (II) and the compound of formula (III) is 1:0.8 to 1.2; the temperature of the reaction is 15-35 ℃.
8. A grease according to claim 3, wherein the reaction is carried out under inert gas protection.
9. A grease according to claim 3, wherein a catalyst is added to the reaction, the catalyst being one or more of a metal phosphine complex, a metal halide and a hydrocarbyl phosphine compound.
10. A grease according to claim 3, wherein a catalyst is added to the reaction, the catalyst being a mixture of a metal phosphine complex, a metal halide and a hydrocarbyl phosphine compound, the molar ratio between the three being 1:0.1 to 10:0.1 to 10.
11. Grease according to any one of claims 1 to 10, wherein the base oil is one or more of mineral oil, vegetable oil and synthetic oil; the thickener comprises one or more of a polyurea thickener, a lithium-based thickener, a composite lithium-based thickener, an amide sodium soap thickener, a calcium-based thickener and a composite aluminum-based thickener; the antirust agent is benzoazole and/or sulfonate antirust agent; the extreme pressure agent is selected from one or more of organo molybdenum, dialkyl dithiocarbamate and amino thioester; the antioxidant is selected from amine antioxidants and/or phenolic antioxidants.
12. Grease according to any of claims 1 to 10, characterized in that the grease comprises 0.1 to 5% of a silole derivative, 75 to 90% of a base oil, 8 to 20% of a thickener, 0.1 to 2.5% of an anti-rust agent, 0.01 to 1% of an antioxidant, 0.01 to 2% of an extreme pressure agent.
13. A method of preparing the grease of any one of claims 1 to 12, comprising: mixing and refining base oil, a thickening agent and the silole derivative, then mixing with the antirust agent, the antioxidant and the extreme pressure agent, and grinding into grease.
14. The method of claim 13, wherein the grease is a complex lithium-based grease; the preparation method of the composite lithium-based lubricating grease comprises the following steps: mixing and heating part of base oil, fatty acid and small molecular acid in a reaction kettle, heating to 40-100 ℃, adding the water solution of the silole derivative and lithium hydroxide, heating to remove water, continuously heating to 190-220 ℃ for high-temperature refining, adding the rest of base oil, cooling to 60-120 ℃, adding the antirust agent, the antioxidant and the extreme pressure agent, and grinding into grease; the fatty acid is C 12 ～C 20 Fatty acids and/or C 12 ～C 20 Hydroxy fatty acid, the small molecule acid is C 2 ～C 11 Is an organic acid of (a).
15. The method of claim 13, wherein the grease is a sodium amide soap based grease; the preparation method of the sodium amide soap-based lubricating grease comprises the following steps: mixing and refining base oil, an amide sodium soap thickener and the silole derivative, mixing with the antirust agent, the antioxidant and the extreme pressure agent, and grinding into grease.
16. The method according to claim 13, wherein the silole derivative is dissolved in a solvent in advance, the solvent being an aromatic hydrocarbon solvent.
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